CN106396618B - A kind of reducing atmosphere fires the manufacturing method of high temperature matt Zijin vitreous enamel - Google Patents
A kind of reducing atmosphere fires the manufacturing method of high temperature matt Zijin vitreous enamel Download PDFInfo
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- C04B33/00—Clay-wares
- C04B33/02—Preparing or treating the raw materials individually or as batches
- C04B33/13—Compounding ingredients
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C8/00—Enamels; Glazes; Fusion seal compositions being frit compositions having non-frit additions
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- C04B33/34—Burning methods combined with glazing
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- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
- C04B41/50—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials
- C04B41/5022—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials with vitreous materials
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- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
- C04B41/81—Coating or impregnation
- C04B41/85—Coating or impregnation with inorganic materials
- C04B41/86—Glazes; Cold glazes
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- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/34—Non-metal oxides, non-metal mixed oxides, or salts thereof that form the non-metal oxides upon heating, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3427—Silicates other than clay, e.g. water glass
- C04B2235/3463—Alumino-silicates other than clay, e.g. mullite
- C04B2235/3472—Alkali metal alumino-silicates other than clay, e.g. spodumene, alkali feldspars such as albite or orthoclase, micas such as muscovite, zeolites such as natrolite
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/658—Atmosphere during thermal treatment
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Abstract
The present invention relates to the manufacturing methods that a kind of reducing atmosphere fires high temperature matt Zijin vitreous enamel, the present invention mainly carries out specific proportion using common natural mineral raw in green body and glaze, the raw materials such as glaze ash, dolomite and coal soil are added in glaze, fire Zijin glaze once under reducing atmosphere at 1280~1320 DEG C, and the shortcomings that unique texture that overcome that existing Zijin glaze glossiness is high, colour generation is uneven, to lack Ming and Qing government porcelain kiln Zijin glaze deep simple and unsophisticated, meet the consumption demand that modern recovers one's original simplicity.Simultaneously, since composition of raw materials is natural mineral raw, production cost is greatly reduced, this not only improves succession and carries forward the outstanding technology in producing porcelain technology of Ancient Times in China, also it is created condition to improve the colour generation quality and stability of traditional ceramics product, therefore has a vast market space.
Description
Technical field
The invention belongs to traditional ceramics manufacturing technology fields, and in particular to a kind of reduction system firing high temperature matt Zijin glaze
The manufacturing method of porcelain, suitable for manufacturing the Zijin glaze household china and decorative ceramics of various top grades.
Background technique
Zijin glaze is one of the outstanding person in ancient times iron series high temperature coloured glaze, is developed to the Song Dynasty, and the purple for determining kiln production is fixed
(what i.e. sauce brown Zijin glaze layer was applied on surface determines kiln ceramic product) stated it is illustrious, by extensive favorable comment and public blueness
It looks at, and valence is high-leveled and difficult seeks, wherein Song Dynasty great writer revives the horizontal bar in the front of a carriage used as an armrest: " the Lushui River public affairs cut the western another name for Sichuan Province of Tea Science, and Dingzhou flower porcelain chisels carbuncle " verse and Ming Dynasty Cao Zhao
" lattice Gu will be discussed ": " purple fixation is purple, has black fixation black as painted, and soil is all white, and it is white fixed that valence is higher than." in " Dingzhou flower porcelain " and " purple
The Zijin vitreous enamel of equally specified kiln production calmly ".Wherein period of Ming and Qing Jing Dezhen Yu Yaochang burns the government porcelain kiln Zijin vitreous enamel made and is even more
Not only there is deep simple and unsophisticated unique artistic glamour, also there is deep cultural connotation and technology connotation abundant.However, due to
Sample is precious, rare, and process recipe is lost, main although correlative study is increasingly subject to extensive concern in recent years
Still concentrate on its art beauty, collect identification and cultural connotation etc., and the content in relation to preparation method and technology
Still it is rarely reported.
In recent years, by scholar at " Jing Dezhen government porcelain kiln Zijin glaze form and in color characteristic " though using energy dispersion X in a text
Luminoscope and colour difference meter more systematically analyze tire, glaze chemical composition and the color of Jing Dezhen Ming and Qing government porcelain kiln Zijin vitreous enamel for the first time
Angle value, the Primary Study composition of different times government porcelain kiln Zijin glaze, formula and be in color characteristic and its immanent cause.To recognize comprehensively
Know Jing Dezhen government porcelain kiln ceramics and intrinsic value, the especially process recipe of Jing Dezhen Ming and Qing government porcelain kiln Zijin glaze, provides one
Fixed scientific material.But the research has carried out network analysis only for the unearthed ancient times Zijin glaze sample of imperial kiln, is not directed to Zijin
The production of glaze and technique recovering research.Though in addition, also there is a small amount of correlative study to report that it is mostly in terms of the preparation of Zijin glaze
Intermediate glaze, and the glaze paint of high gloss can only be burnt under oxidizing atmosphere, it not only cannot achieve what the period of Ming and Qing were generallyd use
Reducing atmosphere is fired, and the deep simple and unsophisticated unique texture of Ming and Qing government porcelain kiln Zijin glaze can not be also restored and present.Such as
In the patent of invention " production method of Zijin glaze " of CN201310116213.6, process for calcining used by Zijin glaze be 1160 ~
1200 DEG C of oxidizing atmospheres are fired, and the appearance of " hand held glittering " is presented.As it can be seen that China is at present with regard to reducing atmosphere
The key technology content for firing high temperature matt Zijin glaze has not yet to see relevant report, and the invention patent technology just can be filled out effectively
Mend this blank.
Summary of the invention
Only have medium temperature oxidizing atmosphere present invention aim to address current Zijin vitreous enamel to fire, and product surface gloss
Height is spent, does not have the technological deficiency of the deep simple and unsophisticated unique texture of ancient times Zijin glaze, it is sub- to provide a kind of reduction system firing high temperature
The manufacturing method of light Zijin vitreous enamel.
In order to solve the above technical problems, the technical scheme is that a kind of reducing atmosphere fires high temperature matt Zijin glaze
The manufacturing method of porcelain, it is characterised in that: use natural minerals for primary raw material, blank raw material by following components by mass percentage
Composition: Yunnan kaolinite 35~50%, southern port porcelain stone 40~60%, potassium feldspar 5~10%；Glaze raw material presses quality hundred by following components
Divide than composition: dolomite 4~10%, coal soil 20~35%, glaze ash 5~15%, glaze fruit 10~20%, quartzy 10~20%, potassium feldspar
15~25%, albite 5~15%, waterglass 0.1~0.2%, through blank raw material and the preparation of glaze raw material, molding, drying, glazing,
Firing obtains matt Zijin vitreous enamel.
The blank raw material preparation section is to weigh raw material by blank formulation requirement and mix, with material: ball: water weight ratio is
1:2:0.6~0.8 is packed into ball-grinding machine ball milling 15~30 minutes, 150 meshes will be crossed after slurry aging 48 hours, using de-
Pug is made in filter, pugging.
The glaze raw material preparation section is to weigh raw material by glaze formula requirement and mix, with material: ball: water weight ratio is
1:2:0.8~1.0 is packed into ball-grinding machine ball milling 20~40 minutes, and fineness reaches 10000-hole sieve and tails over 0.05% or less.
The drying temperature of the drying process is 50 ~ 80 DEG C, and the time is 4 ~ 12 hours.
Glazed thickness control is 0.2~0.6mm in the glazing process.
The firing process includes drying stage, temperature rise period, temperature-fall period, and the drying stage is slow using 1~3 hour
Fire heating, makes kiln temperature degree rise to 500~650 DEG C；The temperature rise period uses oxidizing atmosphere with 2~4 hours first, makes warm in kiln
Degree rises to 980 DEG C and keeps the temperature 0.5~1 hour, then using strongly reducing atmosphere with 1~2 hour, make kiln temperature rise to 1100~
1220 DEG C, finally kiln temperature was set to rise to 1280~1320 DEG C with 0.5~2 hour using weakly reducing atmosphere；The temperature-fall period
To close fire door by kiln natural cooling.
Reducing atmosphere according to the present invention fires high temperature matt Zijin vitreous enamel formula, breaches using oxidizing atmosphere medium temperature
Firing and the bright dazzling limitation of glaze paint colour generation, it is primary raw material that tire glaze formula, which is all made of natural minerals, is passed through using reducing atmosphere
High temperature once-firing, product glaze paint colour generation is deep simple and unsophisticated, and soft glossy affords food for thought, and carcass is fine and close, tire glaze excellent bonding performance,
Thermal stability is good, wide adaptability；Coal soil is introduced in related Zijin glaze formula, has both improved the suspending stabilized of glaze slip
Property, be conducive to glazing, the active iron being uniformly distributed in coal soil further improves the uniformity and stability of glaze paint colour generation, furthermore
Higher aluminium content in coal soil can effectively improve the maturing temperature of glaze, and reduce glaze paint gloss, promote matt effect
Formed, make its can under the conditions of 1280~1320 DEG C high temperature once-firing, improve the appearance of product and the synthesis of product
Performance, therefore have a vast market foreground.
Specific embodiment
Raw mineral materials Yunnan kaolinite used in blank and glaze, southern port porcelain stone, potassium are long in following embodiment of the present invention
Stone, dolomite, coal soil, glaze ash, glaze fruit, quartz, the chemical component of albite are as follows:
Embodiment 1
High temperature matt Zijin vitreous enamel green body body recipe weight percent is that Yunnan kaolinite 45%, southern port porcelain stone 46%, potassium are long
Stone 9%；
High temperature matt Zijin glaze glaze weight percent is dolomite 7%, coal soil 23%, glaze ash 7%, glaze fruit 16%, stone
English 17%, potassium feldspar 17%, albite 12.9%, waterglass 0.1%；
Raw material is weighed by blank formulation requirement and is mixed, and with material: ball: water weight ratio is that 1:2:0.6 is packed into ball-grinding machine ball
Mill 20 minutes will cross 150 meshes after slurry aging 48 hours, pug is made using de- filter, pugging；
Raw material is weighed by glaze formula requirement and is mixed, and with material: ball: water weight ratio is that 1:2:0.8 is packed into ball-grinding machine ball
Mill 28 minutes, fineness reaches 10000-hole sieve and tails over 0.05% or less；
It is made after green body at 50 DEG C 9 hours dry using grouting process, then after dedusting moisturizing by the way of glaze spraying
Glazing is carried out, control glazed thickness is 0.3mm.
It is spontaneously dried after glazing, then uses following calcining system: in drying stage, heated up with 1.5 hours slow fires, make kiln
Interior temperature reaches 550 DEG C, sufficiently excludes moisture contained in product；Again include oxidation stage, restore rank by force in the temperature rise period
Section and weak reduction phase, wherein oxidation stage, was warming up to 980 DEG C with 4 hours, and keep the temperature 0.6 hour, obtains organic matter in base glaze
With fully oxidized decomposition；Strong reduction phase is then continued at, was warming up to 1140 DEG C with 1.2 hours；It is transferred to weakly reducing atmosphere again, with 1
Hour is warming up to 1290 DEG C of firing temperature and makes carcass sintering densification, forms the texture of heavy dense, crystal growth in glaze layer
Development is complete orderly, promotes the formation of surface sauce brown richness iron crystal phase；In cooling stage, fire door is closed by its slow natural cooling
To room temperature.
The surfacing of the present embodiment resulting product, colour generation are uniform, and appearance tone is deep simple and unsophisticated, the matt with soft nature
Artistic effect.
Embodiment 2
High temperature matt Zijin vitreous enamel body recipe weight percent is Yunnan kaolinite 39%, southern port porcelain stone 55%, potassium feldspar 6%；
High temperature matt Zijin glaze glaze weight percent be dolomite 5%, coal soil 31%, glaze ash 11.8%, glaze fruit 12%,
Quartzy 12%, potassium feldspar 21%, albite 7%, waterglass 0.2%；
Raw material is weighed by blank formulation requirement and is mixed, and with material: ball: water weight ratio is that 1:2:0.7 is packed into ball-grinding machine ball
Mill 27 minutes will cross 150 meshes, pug be made using techniques such as de- filter, puggings after slurry aging 48 hours；
Raw material is weighed by glaze formula requirement and is mixed, and with material: ball: water weight ratio is that 1:2:1.0 is packed into ball-grinding machine ball
Mill 36 minutes, fineness reaches 10000-hole sieve and tails over 0.05% or less.
It is made green body uses leaching glaze at 80 DEG C after dedusting moisturizing after drying 6 hours by the way of and is carried out using mechanical pressing
Glazing, glazed thickness 0.5mm.
It is spontaneously dried after glazing, then uses following calcining system: in drying stage, heated up with 2.5 hours slow fires, make kiln
Temperature reaches 630 DEG C, sufficiently excludes moisture contained in product；The temperature rise period include again oxidation stage, strong reduction phase and
Weak reduction phase, is respectively as follows: oxidation stage, was warming up to 980 DEG C with 3 hours, and keep the temperature 0.9 hour, obtains organic matter in base glaze
With fully oxidized decomposition；Strong reduction phase is then continued at, was warming up to 1200 DEG C with 1.8 hours；It is transferred to weakly reducing atmosphere again, uses
It is warming up within 1.8 hours 1300 DEG C of firing temperature and makes carcass sintering densification, form the texture of heavy dense, crystal is raw in glaze layer
Long development is complete orderly, promotes the formation of surface sauce brown richness iron crystal phase；In cooling stage, it is slowly naturally cold by it to close fire door
But to room temperature.
The surfacing of the present embodiment resulting product, colour generation are uniform, and appearance tone is deep simple and unsophisticated, the matt with soft nature
Artistic effect.
Claims (6)
1. the manufacturing method that a kind of reducing atmosphere fires high temperature matt Zijin vitreous enamel, it is characterised in that: based on natural minerals
Raw material is wanted, blank raw material is made of by mass percentage following components: Yunnan kaolinite 35~50%, southern port porcelain stone 40~60%, potassium
Feldspar 5~10%；Glaze raw material is made of by mass percentage following components: dolomite 4~10%, coal soil 20~35%, glaze ash
5~15%, glaze fruit 10~20%, quartzy 10~20%, potassium feldspar 15~25%, albite 5~15%, waterglass 0.1~0.2%, warp
Blank raw material and the preparation of glaze raw material, molding, drying, glazing, firing obtain matt Zijin vitreous enamel.
2. the manufacturing method according to claim 1, it is characterised in that: the blank raw material preparation section is by blank formulation
It is required that weighing raw material and mixing, with material: ball: water weight ratio is that 1:2:0.6~0.8 is packed into ball-grinding machine ball milling 15~30 minutes,
150 meshes will be crossed after slurry aging 48 hours, pug is made using de- filter, pugging.
3. the manufacturing method according to claim 1, it is characterised in that: the glaze raw material preparation section is by glaze formula
It is required that weighing raw material and mixing, with material: ball: water weight ratio is that 1:2:0.8~1.0 is packed into ball-grinding machine ball milling 20~40 minutes,
Fineness reaches 10000-hole sieve and tails over 0.05% or less.
4. the manufacturing method according to claim 1, it is characterised in that: the drying temperature of the drying process is 50 ~ 80 DEG C,
Time is 4 ~ 12 hours.
5. the manufacturing method according to claim 1, it is characterised in that: glazed thickness control is 0.2 in the glazing process
~0.6mm.
6. the manufacturing method according to claim 1, it is characterised in that: the firing process includes drying stage, heating rank
Section, temperature-fall period, the drying stage made kiln temperature rise to 500~650 DEG C using slow fire heating in 1~3 hour；The liter
Thermophase uses oxidizing atmosphere with 2~4 hours first, so that kiln temperature is risen to 980 DEG C and keeps the temperature 0.5~1 hour, then uses
Strongly reducing atmosphere made kiln temperature rise to 1100~1220 DEG C with 1~2 hour, finally small with 0.5~2 using weakly reducing atmosphere
When, so that kiln temperature is risen to 1280~1320 DEG C；The temperature-fall period is to close fire door by kiln natural cooling.
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| CN107285635B (en) * | 2017-08-15 | 2020-08-21 | 马聚魁 | Firewood porcelain bean blue glaze |
| CN107344815B (en) * | 2017-08-15 | 2020-08-18 | 马聚魁 | Green enamel of firewood and porcelain |
| CN111792841B (en) * | 2020-06-15 | 2021-07-30 | 景德镇市正达陶瓷文化传播有限公司 | High-temperature reduction antibacterial ceramic and preparation process thereof |
| CN111848119A (en) * | 2020-07-17 | 2020-10-30 | 怀化市小康瓷砖厂 | Reduction sintering process for double-sided matte glaze green tile |
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| US20070277703A1 (en) * | 2006-06-02 | 2007-12-06 | Iop Specialists Sdn. Bhd. | Iron oxide pigments from mill scale |
| CN102584349A (en) * | 2012-03-27 | 2012-07-18 | 景德镇陶瓷学院 | Iron series colored glazes prepared from chlorite and decoration method thereof |
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| CN102584349A (en) * | 2012-03-27 | 2012-07-18 | 景德镇陶瓷学院 | Iron series colored glazes prepared from chlorite and decoration method thereof |
| CN103224413A (en) * | 2013-04-06 | 2013-07-31 | 湖南益嘉瓷业有限公司 | Producing method of violet gold glaze |
| CN104291870A (en) * | 2014-09-25 | 2015-01-21 | 景德镇陶瓷学院 | Serial ferric colored glaze prepared by using wastewater sludge and decoration method thereof |
| CN105884197A (en) * | 2016-04-07 | 2016-08-24 | 陕西科技大学 | Method for preparing series iron-series colored glaze from iron-ore slag and decoration method based on colored glaze |
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